e415

a ~ull 7INTERNATIONAL Designation: E415-15 Standard Test Method for Analysis of Carbon and Low-Alloy Steel by Spark Atomic Emission Spectrometry 1 This standard is issued under the fixed designation E415; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope according to the design of the spectrometer stand, but a 1.1 This test method covers the simultaneous determination thickness between 10 mm and 38 mm has been found to be of 21 alloying and residual elements in carbon and low-alloy most practical. steels by spark atomic emission vacuum spectrometry in the 1.3 This test method covers the routine control analysis in mass fraction ranges shown Note 1. iron and steelmaking operations and the analysis of processed Composition Range, % material. It is designed for chill-cast, rolled, and forged Applicable specimens. Better performance is expected when reference Element Range, Quantitative Range, materials and specimens are of similar metallurgical condition Mass Fraction Mass Fraction %8 o/oA and composition. However, it is not required for all applica- Aluminum 0 to 0.093 0.006 to 0.093 tions of this standard. Antimony 0 to 0.027 0.006 to 0.027 Arsenic 0 to 0.1 0.003 to 0.1 1.4 This standard does not purport to address all of the Boron 0 to 0.007 0.0004 to 0.007 safety concerns, if any, associated with its use. It is the Calcium 0 to 0.003 0.002 to 0.003 responsibility of the user of this standard to establish appro- Carbon 0 to 1.1 0.02 to 1.1 Chromium 0 to 8.2 0.007 to 8.14 priate safety and health practices and detennine the applica- Cobalt 0 to 0.20 0.006 to 0.20 bility of regulatory limitations prior to use. Copper 0 to 0.5 0.006 to 0.5 Manganese 0 to 2.0 0.03 to 2.0 Molybdenum 0 to 1.3 0.007 to 1.3 2. Referenced Documents Nickel 0 to 5.0 0.006 to 5.0 2.1 ASTM Standards: 3 Niobium 0 to 0.12 0.003 to 0.12 Nitrogen 0 to 0.015 0.01 to 0.055 E29 Practice for Using Significant Digits in Test Data to Phosphorous 0 to 0.085 0.006 to 0.085 Determine Conformance with Specifications Silicon 0 to 1.54 0.02 to 1.54 E135 Terminology Relating to Analytical Chemistry for Sulfur 0 to 0.055 0.001 to 0.055 Tin 0 to 0.061 0.005 to 0.061 Metals, Ores, and Related Materials Titanium 0 to 0.2 0.001 to 0.2 E305 Practice for Establishing and Controlling Atomic Vanadium 0 to 0.3 0.003 to 0.3 Emission Spectrochemical Analytical Curves Zirconium 0 to 0.05 0.01 to 0.05 E350 Test Methods for Chemical Analysis of Carbon Steel, A Applicable range in accordance with Guide E1763 for results reported in accordance with Practice E1950. Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and 8 Quantitative range in accordance with Practice E1601 . Wrought Iron Nom 1-The mass fraction ranges of the elements listed have been E406 Practice for Using Controlled Atmospheres in Spec- established through cooperative testing2 of reference materials. trochemical Analysis E1019 Test Methods for Determination of Carbon, Sulfur, 1.2 This test method covers analysis of specimens having a Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt diameter adequate to overlap and seal the bore of the spark Alloys by Various Combustion and Fusion Techniques stand opening. The specimen thickness can vary significantly E1329 Practice for Verification and Use of Control Charts in Spectrochemical Analysis E1601 Practice for Conducting an Interlaboratory Study to 1 This test method is under the jurisdiction of ASTM Committee EO! on Evaluate the Performance of an Analytical Method Analytical Chemistry for Metals, Ores, and Related Materials and is the direct E1763 Guide for Interpretation and Use of Results from responsibility of Subcommittee EOI.OI on Iron, Steel, and Ferroalloys. Current edition approved Nov. 15, 2015. Published March 2016. Originally approved in 1971. Last previous edition approved in 2014 as E415- 14. DOl: 10.1520/E0415-15. 3 For referenced ASTM standards, visit the ASTM website, www.astrn.org, or 2 Supporting data have been filed at ASTM International Headquarters and may contact ASTM Customer Service at [email protected]. For Annual Book of ASTM be obtained by requesting Research Report RR:EOl-1122. ContactASTM Customer Standards volume information, refer to the standard's Document Summary page on Service at [email protected]. the ASTM website. Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States ASTM International. ASTM See 11. 6.3 A hybrid design using both photomultipliers and carbon.1. 5. 7 . The measuring Chart Analysis 5 system may consist of one of the following configurations: 3. Significance and Use keep the 0 2 (g) residual <500 ng/g and H2 0 (g) residual <1 ~g/g and remove impurities of nitrogen and hydrocarbons. Spectral lines other than E2972 Guide for Production. and the relative radiant energies of the analytical register the voltage of said output ports.1 Refer to Practice E1806 for devices and practices to 7. it should be capable and alloys is primarily intended to test such materials for of maintaining a vacuum of 3. 6.1 A black deposit will collect on the tip of the electrode. ground surface of the disk specimen and a conically shaped pixel selection electronics to reset the pixels and to transport electrode. lines are recorded. 7. and tin lie in the vacuum semiconductor arrays.1 This test method for the spectrometric analysis of metals If the instrument is using a vacuum pump.org. Apparatus flow rate may be manually or automatically set.2 Excitation Source. The absorption of the radiation by air in this 6. safely. silver or thoriated tungsten rods. The spectrom- El950 Practice for Reporting Results from Methods of eter must be able to measure at least one of the listed spectral Chemical Analysis lines for each of the listed elements. The argon 6. Summary of Test Method vide the desired sequence of operation.23 m3 /min (8 performing common laboratory procedures skillfully and ft 3/min) is usually adequate.2 Other ASTM Documents 6. on a thoriated tungsten electrode before replacement is necessary.5. The rods can vary in diameter from 1.5 mm to 6.1. ASTM International. 4. It is assumed that all who use this test method will be analysts capable of NOTE 2-A pump with a displacement of at least 0. 2 Copyright ASTM International.5. and Value Assignment those listed in Table 1 may be used provided it can be shown of In-House Reference Materials for Metals. nitrogen. 2. E1806 Practice for Sampling Steel and Iron for Determina.Tel : +49 30 2601-2361 . During continuous operation. and a voltage measuring system to mined time. automatically flushed with argon. cO E415-15 Interlaboratory Testing of Chemical Analysis Methods (verifier data or other reference sample intensity data can (Withdrawn 2015)4 typically indicate when this is necessary). and experimentally that equivalent precision and accuracy are Other Related Materials obtained. phosphorus. provided it rameters to spark a sample. ultraviolet region.1 Follow the manufacturer's recommendations for This deposit should be removed between specimens (typically cleaning the spark chamber.1 Sampling Devices: system shall be in accordance with Practice E406. compliance with compositional specifications. If not removed. or at a predeter. it can reduce the overall typically should be done every 24 h. Terminology 6.2 A semiconductor detector array (CCD or CMOS). 6. spectrometer capable of converting ASTM MNL 7 Manual on Presentation of Data and Control light intensities to measurable electrical signals. can be shown experimentally that equivalent precision and bias 6.3 Spark Chamber. Follow the manufacturer's intensity of the spectral radiation or transfer slight amounts of recommendations for cleaning the entrance lens or window contamination between specimens. It may be necessary to have a gas purification system spark chamber with argon. or both.7 Gas System.1 for details. 4 The last approved version of this historical standard is referenced on www. and the necessary switching arrangements to pro- 4.3.5.33 Pa (25 ~ Hg) or less. It is expected that work will be performed in a properly 6.1 For definitions of terms used in this test method. or other material. boron.1 A photomultiplier (PMT) array having individual voltage adjustments.5 Measuring System. consisting of a circulation pump and a cleaning cartridge to 5. 8th edition. Reagents and Materials sample liquid and solid iron and steel. and should be established in each laboratory. Automatic sequencing shall be provided to actuate the flow at a given rate for a specific time interval. capacitors in which the output of each 3. Nom 3-lt has been reported that thousands of burns can be performed 5 ASTM Manual Series. Testing.5 spark chamber shall be mounted directly on the spectrometer mm (depending on the instrument design) and typically are and shall be provided with a spark stand to hold a flat specimen machined to a 90° or 120° angled tip. 6. The number of acceptable burns on an electrode varies from one instrument to another. check the manufacturer's suggested gas a vacuum ultraviolet (VUV) transparent gas and flushing the purity.1 A capacitor discharge is produced between the flat. of the detector arrays.4 Spectral Lines-Table 1 lists spectral lines and internal tion of Chemical Composition standards usable for carbon and low alloy steel.6 Optical Path-If the instrument is operated using a region is overcome by evacuating the spectrometer or by use of VUV transparent gas. capable of providing electrical pa. 2010. sulfur. and flow regulation. The most sensitive lines of arsenic.1 Counter Electrodes-The counter electrodes can be 6. register the voltages on the capacitors either directly or indirectly. The are obtained. Ores. this with a wire brush). Distributed under ASTM license by Beuth Verlag. 6. a voltage measuring system to TerminologyE135 . and a lower counter electrode of rod form. The 6. consisting of an argon supply with pressure equipped laboratory. refer to photomultiplier is stored.astm. The discharge is terminated at a predetermined the voltage of an individual pixel to one or more output ports intensity time integral of a selected iron line. Mo.64 I S. W 193.55 w 136.26 W. Mo.72 II Mn.59 3 ASTM license by Beuth Verlag. Mn Antimony 217.76 235.63 363. W Cobalt 345.92 II Mn.33 487.34 182.59 I W.20 Mo. Mo 182.62 II Ni. Line Possible Element A.14 157.79 517. Mn.83 339.03 II Fe.12 239.09 AI Chromium 312..33 249. Nb.24 174.65 226. Cr 197.04 V.13 II 182.05 299. Mo 267.74 304.93 328.35 I Cr.33 285.22 V. Ni.91 316. Mn.69 297.37 282. Ni 308.75 Mn. Nb 327.20 217. Cr 510.76 Mn Boron 345.26 II v 313. nm ClassificationA lnterference 8 Aluminum 396.75 383.Tel : +49 30 2601-2361 .81 303. Mn.81 Cr 193.21 281 . Cr 258. Nb. Cu Calcium 393.76 Iron (IS) 305. V.44 I 298.40 V. Mn.85 II Nb Carbon 165.28 179. W Arsenic 189. Mo 228.40 172.15 Mo 394.18 296.21 458.95 300.81 218.21 II 425.40 Nb 224.3 Si 324.88 205.60 Mo.38 413.15 277.16 321 . W Copper 212.68 308.70 410.6 Ni.13 216. Mn.37 II 396. cO E415-15 TABLE 1 Internal Standard and Analytical Lines Wavelength.Ni 213. Si. V Nitrogen 149.V.07 Co 492.65 271. Cu. nm ClassificationA lnterference 8 226. and excitation conditions. Ni.73 Mn Tin 147.26 Fe. W 243.75 149.19 II w A The numerals I or II in the line classification column indicate that the line has been classified in a term array and definitely assigned to the normal atom (I) or to the singly ionized atom (II). cO E415-15 TABLE 1 Continued Wavelength.61 Fe. 4 Copyright ASTM International. Ni and nitride forming elements such as 1i Phosphorus 178..99 II 1i. Cu. Cu. Mo. 1i 227.41 I V.44 273.88 I 202. Co 337.20 II Nb 400. Mn 281 .Cr.73 II 341 .75 Mn Manganese 293.48 I 352. W.50 II Co Vanadium 437. V.54 I Cu. Line Possible Element A. Ni Zirconium 468.08 II 1i.16 Mo.V 319.AI. spectrum line choices.29 Mo Silicon 288. 1i.Mn 220.55 Cr. Nb.62 II 343. and those listed require confirmation based upon specimens selected especially to demonstrate suspected interferences.03 II 277. Mo. Ni Niobium 313. Fe.23 II Fe. V 212. 1i Sulfur 180. V.Tel : +49 30 2601-2361 .86 II Zr 263.82 II w 206.92 I 310.99 II Mn.61 II Mn 386. AI Titanium 308. Nb 390.82 II AI. 8 Interferences are dependent upon instrument design.48 187.44 I 227. W 251 .52 II 189. Mo. Ni 255.28 II Nb Tungsten 324.41 Mo.79 II Co. Cr Nickel 471.83 II Mn 202.31 II Cr. Co.53 190. Distributed under ASTM license by Beuth Verlag.78 I 349.W Molybdenum 379.50 II Mo.20 193.45 I 231 .76 218.65 216.39 Lead 405.60 II Co. Mn.80 I Cu.02 II Nb. Initially. This shall be done initially and as often as necessary to Guide E2972 for production of your own reference materials. and the frequency of use. with a 50-grit to 80-grit abrasive belt or disc (wet or dry) or 11. It is 11." lines and one of the analytical lines for each element listed in 8. Typical samples position of the exit slits will depend on factors such as the type of can be used to determine repeatability of individual measure.3 to 0. 120-grit) may be used for the final grind. particular spectrometer. The laboratory will deter- 8. causing low results. 9. cO E415-15 7. Therefore.1 Reference materials and specimens shall be refinished dry on an abrasive belt or disc before being remeasured on the 8. 11. and distributions of inclusions. n 2. Capacitance. spectrometer.1 Electrical Parameters: recommended to validate results using typical samples ana.1. IJH 50 to 70 in the same manner. and in drift correction (standardization) of the spectrometer. However. 8. and they may be useful in calibrations.1 Burn parameters are normally established by the lyzed using Test Methods E350 and E1019.1.2 When parameter values are established. refer to the manufacturer's manual(s). calibrations may be biased. further exit slit alignment is not neces- individual measurements of elements found in the inclusions. IJF 10to 15 9. sary (Note 7). Follow the manufac- turer's recommended procedures. spectrometer manufacturer. The following ranges are historical guidelines and newer instruments may vary from these: 9. maintain proper entrance slit alignment. IJH residual Nam 5-Specimen porosity is undesirable because it leads to the Resistance. The variation of the power supply voltage shall the region to be measured (Note 5). r-f 0. It is not within the scope of an ASTM test method to prescribe the performance of the test method. Argon. "Standard Reference Material. Multiple lines may be used for a given element (for multiple suppliers or can be developed in house. Distributed under ASTM license by Beuth Verlag. They are used to calibrate the modification.1 The specimens and reference materials shall be prepared Inductance. perform the final grind with a shall be adequate to uniformly trigger the capacitor discharge. and electron emission is inhibited by oily. and additional preparation of the equipment may be re- spectrometer for the elements of interest or to validate the quired. The specimen surface should be kept clean because the specimen is the electron emitter. Preparation of Apparatus Nam 6---The instructions given in this test method apply to most (NIST) and other sources and span all or part of the mass spectrometers. n 3 to 5 Potential. These reference 10. grind the surface not exceed ±5% and preferably should be held within ±2 %. Preparation of Specimens and Reference Materials Triggered Capacitor Discharge Capacitance. It is not recommended to use minute details of the apparatus preparation. A finer abrasive grinding media (for The following settings are historical guidelines and newer example.5 improper "diffuse-type" rather than the desired "concentrated-type" dis. Refer to ber. samples.3 are not 5 Copyright ASTM International.1. Burn and Exposure reference materials with metallurgical structure similar to typical samples.1 and 11. 11. compositions.1. on surfaces.1. nickel) depending on the mass fraction range and the Materials are typically used in control procedures (verifiers) individual spectrometer software. which may differ not only for CRMs as verifiers or to establish the repeatability of the each manufacturer. V 940 to 1000 section shall be of sufficient size and thickness for preparation Current.1. dirty 11.3 Exit slit positioning and alignment is normally per- sizes.2 Ensure that the specimens are free from voids and pits in them carefully.1 Certified Reference Materials (CRMs)-These are avail- able from the National Institute of Standards and Technology 10.Tel : +49 30 2601-2361 .3 Initiation Circuit-The initiator circuit parameters mill the surface.2 For certain elements. Some inclusions may be removed during preburn steps prior to Nom 7-The manner and frequency of positioning or checking the integration of intensities.3. For a description of and further details of operation for a chemical measurement process. Reference Materials same area.2 Test the positioning of the spectrometer entrance slit to materials shall be homogenous and contain appropriate mass ensure that peak radiation is entering the spectrometer cham- fractions of each element for the intended purpose.1 Samples and reference materials may exhibit differ- ences in metallurgical structure. the variety of analytical problems encountered. If wet grinding. 8. in particular having different 10. A specimen cut from a large sample Resistance. V 18 000 charge. 8.8 and to properly fit the spectrometer stand.1 Program the spectrometer to use the internal standard trademarked with the name.4 Other Electrical Parameters-Excitation units. Peak voltage.3 Several issues can impact the selection and use of mine the frequency of positioning the alignment based on CRMs and RMs: instrument performance. but is not instruments may vary from these: essential.2. Nom 4---Certified Reference Materials manufactured by NIST are 10. Inhomo.2 Reference Materials (RMs)-These are available from Table 1. Each laboratory should establish a suitable check ments to yield estimates consistent with performance for actual procedure utilizing qualified service engineers.2 Inert Gas.1. Under geneous distribution of inclusions can worsen repeatability of normal circumstances. which the precise parameters given in 11. A. IJF 0. formed by the manufacturer at spectrometer assembly. there may be no available 11. Reference example.0025 Inductance.3. but also for different equipment from the same manufacturer. in accordance with Practice E406. A 10-mm to 38-mm Number of discharges 60 thick specimen is normally most practical. dry abrasive belt or disc. maintain 9. some settings and adjustments may require fraction ranges listed in 1. 2 Burn and Measurement Conditions-The following instrument manual or instrument manufacturer for access to ranges are normally adequate: this information. Distributed under ASTM license by Beuth Verlag. white burn without the characteristic dark 11. unless an alternative rounding method is speci- verifier two times to four times and use the average value.4 Photomultiplier Potentials-The sensitivities of the approximately 6 mm (1/4 in.2. or 5 mm (±0. If Flush 5 to 45 2.) There shall be at least three 14. s 5 to 15 12.1 Using the average results obtained in 13. may be used provided that it can be shown experi. measure calibrants and potential drift correction samples 14. Use either a 3 mm.2 A high-purity argon atmosphere is required at the within the control limits established in 12.1. Refer to your 11. standardize on an initial setup or anytime that it is known or suspected that readings have shifted. drift correction sample. offsets are often presented in the spectrometer software after mentally that equivalent precision and accuracy are obtained. Calculation 12. If boron nitride disks are semiconductor detector arrays are replacing PMTs.1 Select preburn and exposure periods after a study of 12.2 Precision-Up to eight laboratories cooperated in per- the necessary corrections either by adjusting the controls on the forming this test method with thirteen unknown samples and readout or by applying arithmetic corrections. 4 mm.Tel : +49 30 2601-2361 . usually exhibits a dark ring around the pitted sparked area.1 Supporting data have been filed atASTM International Practice E305 . 90° or 120° angled cone. Measurements with two bums to six bums using the operating conditions described in 11.1 and 11. Precision and Bias averages of the data for each point.3. In the case of automatic mined by this method and the certified compositions provides corrections conducted by the spectrometer software. a properly burned specimen may not exhibit a dark ring.5 to 15 run another standardization or investigate why the instrument may be malfunctioning.1. Practice E1329. Preburn 5 to 45 2.Z The interlaboratory test data summarized in Table 2 12. Using the 15. serves as one electrode. hydrocarbons.2 Rounding of test results obtained using this test method calibrants for each element.1 Analyze verifiers in accordance with Section 13. such as nitrogen. quency of verification based on statistical analysis.1 - 11. Standardization. s 5 to 20 tion is valid immediately after each standardization and as Exposure period. Standardization obtained the statistical information summarized in Table 2. Typically maintain the parameters consistently.2. Argon flow ft 3 /h Umin 12. perform a stan- analytical gap.3 Electrode System-The specimen.2. 13. should be minimized. spanning the required mass frac. s 3 to 30 required in accordance with 12.1 mm) analytical gap. or other equivalent tungsten or silver rod.2. Measure each calibrant. With that equipment. used later as a verifier. the tip of which has been machined to a quality control procedure. observe the bias found in the interlaboratory study.) from the edge of the specimen. every 4 h to 8 h is practical and adequate.2. repeat with different random sequences at least two times. 12. the spectrometer system and software permit.2 Standardization-Following the manufacturer's have been evaluated in accordance with Practice E1601.3 Verification-Verify that the instrument's standardiza- Preburn period. Headquarters and may be obtained by requesting RR:E01- 1122. Bias information is the standardization factors and/or offsets. either in the gas system necessary so verification results are within control limits or or from improperly prepared specimens. See 8.2 Measure specimens in duplicate and report the average of the duplicate results.1 Calibration-Using the conditions given in 11.5 to 25 Exposure 5 to 30 2. and Verification 14. 11. electrically 12. The factors and/or found in Table 2. Condition a fresh counter electrode 13. 6 Copyright ASTM International. If the results are not 11. (A calibrant may be developed in 12. If fied by the customer or applicable material specification. Repeat standardization as oxygen. Molecular gas impurities. Once established. bracketing these with measurements of the mass fractions of the elements from the analytical curves any materials intended for use as verifiers. Calibration. a properly burned specimen selected.5 Semiconductor Detector Array-In newer instruments ring indicates an improperly burned specimen. a smooth texture. standardization and/or stored in log files. shall be done anytime verification indicates that readings have 15.4. photomultipliers are normally established and set by the spectrometer manufacturer based on the particular wavelengths NoTE 8-With certain spectrometers.1 Place the prepared surface of the specimen on the sample stand so that measurement shall impinge on a location 11. The opposite electrode is a dance with ASTM MNL 7. dardization and repeat verification. Make 15.3 Bias-Differences between average composition deter- gone out of statistical control.3. The width used to mechanically restrict the burned area of the sample. recommendations.3.3. 11. and Practice E29.4 Quality Control-Establish control limits in accor- negative. shall be performed in accordance with the Rounding Method of tion range. calculate in a random sequence.2 Each laboratory shall determine the necessary fre- volatization rates during specimen bums. Argon flush period.5 to 25 results do not fall within the control limits established in 12. investigate further for instrument problems. of the individual pixels shall be similar to the width of the exit slits used in conventional instruments equipped with PMTs. or water vapor. determine analytical curves as directed in the spectrometer manufacturer's software or 15.4. 13. cO E415-15 available. 0116 -0.016 0.0014 0.0001 Sample 7 8 0.0002 0.0005 Sample 9 4 0.0005) 0.0201 0.0001 0.0001 0.003 0.0035 0.002 0.05 0.0004 Sample 4 8 (<0.0008 0.0196 -0.0004 0.0010 0.0009 0.0333 0.0009 0.004 0. cO E415-15 TABLE 2 Statistical Information Number of Certified Material X bar R Bias Laboratories Value.0043 0.0012 0.0001 0.0015 Sample 7 7 (0.0001 0.0007 0.0011 0.0008 0.142 0. Distributed under ASTM license by Beuth Verlag.0009 0.0890 0.0037 0.0200 0.0459 0.0021 0.0003 Sample 2 4 (0.005) 0.0012 0.0059 Sample 2 7 0.1525 0.0006 0.0175 0.0001 0.0033 0.0005) 0.041 0.0010 0.0010 0.0011 Sample 10 8 0.0256 0.0098 0.0031 Sample 13 7 0.0286 0.0002 0.0071 0.0003 0.0022 Sample 4 6 0.0001 0.0008 0.0002 Sample 6 7 0.027 0.0152 -0.0002 Sample 8 7 0.0002 0.0014 Sample 7 8 0.0067 0.0003 Sample 9 5 0.0012 0.0000 0.0001 0.0076 0.0002 Sample 10 7 0.0004 0.0048 Sample 8 6 0.Tel : +49 30 2601-2361 .0003 0.0000 0.0004 Sample 9 6 0.0018 0.0044 0.0008 0.0009 0.0174 0.0007 0.0004 0.0167 0.0002 Sample 3 8 0.0001 0.0002 Calcium Sample 1 3 (<0.0015 Sample 2 7 0.0048 Sample 6 8 0.0024 0.0002 0.0001 0.0003 0.0252 0.0230 O.0037 0.0002 Sample 13 7 0.0001 0.0003 0.0005) 0.0065 0.0022 0.017 0.0003 0.0272 0.0015 0.0002 Sample 5 4 (<0.0002 Sample 2 7 (0.0002 Sample 2 5 0.0028 0.0011 Sample 11 6 0.0005 0.0016 Sample 12 8 0.0001 0.0026 0.0017 0.0017 0.0052 0.0001 0.0008 0.0031 0.0024 0.0654 0.0027 Antimon Sample 1 7 0.001) 0.0022 Sample 5 6 0.0001) 0.0002 Sample 12 3 (0.018 0.0008 -0.0004 Sample 9 7 0.0004 0.0002 Sample 8 5 0.0004 Carbon Sample 1 7 0.211 0.0007 Sample 6 8 0.0046 Boron Sample 1 4 (0.0004 0.0035 0.0009 Sample 5 7 0.0010 0.0234 0.007 0.1384 0.0002 0.0001 Sample 3 8 0.0668 0.2169 0.0047 0.0077 0.0047 Arsenic Sample 1 6 0.0037 0.0002 Sample 5 7 0.0006 0.0014 0.13 0.0073 0.0001) 0.0034 0.0056 0.0024 0.0084 7 Copyright ASTM International.0012 Sample 3 7 0.006 0.0005 0.0006 Sample 13 7 0.0037 0.0028 Sample 13 7 0.0006 0.005) 0.0072 0.0008 0.0013 0.0015 0.0005 0.0020 -0.0045 0.027 0.0014 0.015 0.0003 Sample 4 6 (0.0001 0.0009 0.0001 0.03 0.0050 0.0001 0.0002 Sample 11 8 0.0084 0.0034 Sample 10 7 0.0001 0.0002 Sample 6 8 0.0002 0.0032 0.0047 0.003 0.07 0.0074 0.0010 0.0000 Sample 7 8 0.0001 Sample 11 6 0.0002 Sample 6 8 0.0040 Sample 8 7 0.0001 0.0037 -0.00002) 0.0007 0.0002) 0.0053 0.0003 Sample 3 7 0.0003 0.0002 0.0004 Sample 10 7 0.0023 0.0006 Sample 12 7 0.0009 Sample 13 6 0.0042 0.0002 0.% Aluminum Sample 1 7 0.007 0.0003 0.0003 0.0014 0.0026 0.0002 0.0004 Sample 12 8 (0.0024 Sample 12 8 0.0001 0.0003 Sample 3 8 0.0004 Sample 8 7 0.0012 0.002 0.0111 0.0004 0.0012 0.0006 0.0002 0.0062 0.0008 0.0011 0.0016 Sample 11 8 0.0008 0.0025 0.021 0.0020 Sample 5 8 0.0024 Sample 4 8 0.062 0.0031 0.0029 0.0003 0.0001 0.0001 Sample 7 8 0.0001 0.0009 0.0007 0.0008 0.D105 Sample 3 8 0.0013 Sample 11 7 0.0019 0.0011 0.0024 Sample 9 7 0.024 0.0033 0.0041 Sample 2 6 0.0000 0.093 0.0028 0.0004) 0.0003 0.0033 Sample 10 8 0.0079 0.0001 0.0008 0.0001 0.0413 0.0041 0.0001 0.0022 -0.0002 -0.0031 0.0024 0.0047 Sample 4 7 (<0. 006 0.12 1.0058 0.0093 0.062 0.0040 0.0202 0.019 0.0217 -0.0001 Man anese Sample 1 7 0.55 0.12 0.08 0.0132 0.044 0.4687 0.0226 0.0008 0.4549 0.0028 0.0076 0.8070 0.0061 -0.0043 Sample 4 8 0.05 0.56 2.0070 Mol benum Sample 1 7 0.0033 -0.0084 Sample 10 8 0.0044 Sample 13 7 0.0023 Sample 8 7 0.0013 Sample 2 7 0.0001 Sample 6 8 0.021 0.0011 Sample 8 7 O.0083 0.0101 0.0176 0.0058 -0.0004 Sample 10 8 1.0402 0.0009 0.82 0.0047 0.0002 0.0072 0.0045 0.0000 Sample 13 7 0.0009 0.0051 Sample 4 8 0.148 0. Distributed under ASTM license by Beuth Verlag.0014 Sample 5 8 0.0789 0.22 8.0002 0.0033 0.483 0.0019 0.1196 0.107 0.0017 Sample 3 8 0.0417 0.024 Sample 8 7 2.051 0.0003 Sample 3 8 0.115 0.0255 -0.0142 -0.0167 Chromium Sample 1 7 0.0026 0.128 0.44 0.557 0.0028 -0.0146 0.0033 0.003 Sample 10 8 1.1564 0.0006 0.0227 -0.0036 Sample 5 8 0.028 Sample 3 8 0.0006 Sample 4 8 0.457 0.0006 Sample 12 8 0.0096 0.0012 0.1151 0.025 Sample 12 8 0.0034 0.47 0.255 0.0009 0.Q105 Sample 7 8 0.0001 Sample 5 8 0.0040 Sample 13 7 0.095 0.098 0.3534 -0.1114 0.0003 Sample 10 8 0.0030 0.3593 0.0034 0.0009 0.027 8 Copyright ASTM International.0133 -0.8918 -0.0072 0.01 0.0517 0.151 0.0327 0.0298 O.0035 -0.0051 0.36 1.0797 0.0075 0.0027 Sample 9 7 0.0911 -0.332 0.0040 Sample 11 8 1.0061 0.1784 0.8 0.143 0.0190 0.0011 0.106 0.0029 Sample 10 8 0.3374 0.0022 -0.0033 0.0116 0.7825 0.0039 0.081 0.0280 0.0160 0.0003 Sample 7 8 0.0075 0.0066 0.0170 0.0034 0.0051 0.0116 0.0104 0.4743 0.6605 0.0551 0.658 0.005 0.441 0.3340 0.0280 -0.09 2.3209 -0.0008 Sample 5 8 0.0221 0.0204 0.0031 0.0028 -0.0008 Sample 11 8 0.0832 0.0088 0.0020 0.0200 0.0007 Sample 7 8 5.0007 Sample 2 7 1.0002 Sample 7 8 1.22 4.0006 0.0038 0.0025 Sample 5 8 0.33 0.0270 0.03 0.006 Sample 11 8 0.0083 0.0020 0.0016 0.Tel : +49 30 2601-2361 .0019 0.0569 0.445 0.0168 0.0156 0. cO E415-15 TABLE2 Continued Number of Certified Material Xbar R Bias Laboratories Value.0025 Sample 9 7 0.0026 -0.0444 0.0005 Sample 6 8 0.0014 Sample 9 7 0.0039 0.0265 0.0254 0.0066 -0.0231 0.0092 0.0071 0.0078 0.0419 0.0145 0.0103 -0.0161 0.0009 0.1518 0.7330 0.0097 0.0014 0.0013 0.0030 Cobalt Sample 1 7 0.0070 0.0068 0.0001 Sample 2 7 0.086 0.0131 0.4892 0.0041 0.0124 0.0020 Sample 6 8 0.2530 0.2993 0.023 0.316 0.3334 0.299 0.0130 -0.11 0.0169 0.005 Sample 9 7 2.0009 0.0373 0.209 0.16 0.0009 0.005 0.0339 0.0137 -0.0117 Sample 7 8 0.0081 0.333 0.8319 0.34 0.0037 0.Q1 0.0039 Sample 3 8 0.0030 0.11 5.0432 0.169 0.0115 0.0511 0.0007 0.42 1.0034 0.356 0.28 1.0251 0.1190 0.0017 Sample 2 7 0.0167 0.0020 Sample 12 8 0.0044 Sample 13 7 0.03 1.0045 0.077 Sample 13 7 0.0069 Sample 8 7 0.4437 0.72 0.1305 0.0650 0.016 0.015 0.0050 0.024 0.3153 0.0002 Sample 11 8 0.0032 Co er Sample 1 7 0.1885 0.0083 0.0415 0.0049 0.0006 0.011 Sample 4 8 0.0032 -0.0163 0.0081 0.1200 0.0066 Sample 12 8 8.1249 -0.0015 Sample 2 7 0.0009 0.177 0.0023 0.0006 Sample 7 8 0.004 Sample 11 8 0.0062 Sample 6 8 0.11 0.0336 0.0025 -0.011 0.008 0.0075 0.0001 Sample 8 7 0.0004 Sample 9 7 0.% Sample 4 8 0.3251 0.0095 0.1094 0.057 0.0004 Sample 3 8 4.0025 0.376 0.0024 0.0091 0.19 0.0279 -0.772 0.0119 Sample 5 8 0.0110 0.0024 0.0182 0.5584 0.007 0.0079 -0.0026 0.0007 Sample 12 8 0.0130 0.0004 0.0011 0.0797 0.0012 Sample 6 8 0.0149 Sample 4 8 0.0130 Sample 6 8 0.0033 0.1068 0.0007 0.0973 0.0032 -0.1713 0.005 0.307 0. 0033 0.0008 0.0068 0.0023 Sample 2 7 0.163 0.25 0.0119 0.0564 0.0228 0.002) 0.02 1.061 0.0084 0.0008 0.013 0.008 0.0050 -0.0029 0.0007 -0.011 0.0048 -0.002 0.0071 0.0097 0.0018 0.0010 0.0009 Sample 9 7 0.0094 -0.0027 0.154 0.0022 Nickel Sample 1 7 0.2111 0.0237 0.0036 0.0096 0.0003 0.0033 Sample 7 8 0.01 0.0024 0.0011 0.0013 0.0163 0.0040 0.0009 Sample 11 8 0.0100 -0.42 0.123 0.0105 -0.0044 0.0170 0.0228 0.0330 -0.32 0.0013 0.0694 0.4210 0.4486 0.024 0.0007 0.0014 Sample 2 7 0.0005 0.0008 0.1032 0.8976 0.0078 0.2498 0.2787 0.0005 Sample 9 7 0.0102 0.1356 0.0064 0.0064 0.0008 0.0005 Nitro en Sample 1 7 0.0003 0.0075 0.0003 0.035 0.0215 0.3217 0.0074 0.0023 Sample 3 8 0.0006 Sample 11 8 1.0048 0.0007 0.0026 Silicon Sample 1 7 0. cO E415-15 TABLE2 Continued Number of Certified Material Xbar R Bias Laboratories Value.0798 0.0012 0.0008 0.0144 Sample 9 7 1.0105 -0.0005 Sample 5 5 (<0.74 1.1213 0.0039 0.0057 0.012 Sample 12 8 0.0115 0.0003 0.0116 0.1978 0.015 0.0008 0.0867 -0.0009 0.0048 Sample 4 6 0.0007 0.0004 Sample 6 8 0.0034 Sample 11 8 0.015 0.5 0.1573 0.0020 -0.0023 0.0074 0.0022 Sample 12 8 0.9 0.0029 Sample 5 8 0.0043 0.0612 -0.0013 0.0149 Sample 6 8 0.0014 Sample 13 7 0.018 0.0127 0.0146 0.32 0.0013 0.0117 0.0071 -0.0094 0.0076 0.12 0.0028 0.9044 0.006 0.43 0.0020 0.0064 Sample 10 8 0.445 0.0048 -0.255 0.0018 0.0009 0.0684 0.0010 Sample 2 7 0.775 0.54 1.0016 Sample 2 7 0.0088 Sample 3 8 0.0034 0.21 0.3211 0.041 0.0017 Sample 11 8 1.0010 0.012 0.0112 0.519 0.0036 Sample 8 7 0.197 0.0004 0.24 0.0012 Sample 10 8 0.0004 Sample 8 7 0.0018 Sample 8 7 0.135 0.0839 0.0006 Sample 6 7 0.015 Sample 10 8 0.0157 0.0006 0.0099 0.0103 0.0564 0.0011 Sample 10 8 0.0088 0.0030 0.0002 Sample 10 8 0.016 0.0106 0.0183 0.0008 0.0005 Sample 7 8 0.0035 0.0012 0.0363 0.0159 0.0003 0.0019 0.0018 Sample 10 8 0.0490 -0.0128 0.0052 Sample 5 8 0.0009 0.0215 -0.0029 Sample 9 7 0.0017 -0.0041 Sample 5 8 0.0053 0.0011 Sample 7 8 0.01 0.0051 0.0019 -0.0011 Sample 4 8 0.0584 0.0026 0.0006 0.018 0.0010 0.0004 Niobium Sample 1 7 0.0217 0.0116 0.0031 0.0007 0.0347 -0.0003 0.0018 Sample 9 7 0.0016 Sample 6 8 0.0021 0.044 0.055 0.0074 0.0044 0.0008 Sample 11 8 0.029 0.0153 -0.0015 Sample 11 8 0.2520 0.0010 0.0078 0.069 0.4959 0.0245 0.0071 0.0087 Sample 4 8 0.0026 Sample 3 8 0.2251 0.0139 0.0003 0.0101 0.0036 0.0111 0.0029 -0.2 0.Tel : +49 30 2601-2361 .0054 0.0055 -0.0088 0.0090 Sample 4 8 0.0002 0.0090 0.0209 Sample 8 7 0.0005 Sample 3 8 0.0012 0.0106 0.27 0.0684 0. Distributed under ASTM license by Beuth Verlag.% Sample 8 7 0.0030 Sample 9 7 0.003 0.0005 Sample 12 6 0.0079 Sample 13 6 0.0091 0.0043 -0.1999 0.0005 0.0031 0.0044 Sample 4 8 0.0043 0.0164 0.0002 Sample 5 8 0.0010 Sample 12 8 0.0087 0.0056 0.021 9 Copyright ASTM International.0668 0.0004 Sample 7 8 0.0056 0.0001 Sample 2 7 0.0066 0.0022 0.0159 0.017 0.0021 0.0099 0.122 0.89 0.0019 0.0010 Sample 6 8 0.0004 0.011 0.4286 0.0567 0.0233 0.0168 0.0047 -0.0017 Sample 13 7 0.728 0.076 0.0015 0.0083 0.0042 Sample 8 7 (<0.0101 0.1178 0.0034 0.0021 0.003) 0.0448 0.1682 0.058 0.0024 Sample 13 7 0.0415 0.0117 0.0031 -0.0228 -0.0178 -0.01 0.0051 Phos horous Sample 1 7 0.0002 0.0007 Sample 7 8 0.0316 0.0013 Sample 12 8 0.0010 0.0050 Sample 3 8 0.7541 0.0129 0.0006 0.1290 0.0002 Sample 13 7 0. 0005 0.0124 0.0005 0.0009 Sample 8 7 0.0062 0.001) 0.0002 0.006 0.0010 0.0001 0.0023 -0.0014 Sample 6 8 0.0075 0.0011 0.0036 0.013 0.0026 0.003 0.003 0.012 0.0007 0.3116 0.0112 0.0001 0.008 0.0004 Sample 3 8 0.0014 Sample 6 8 0.0190 -0.0454 0.014 0.0016 0.0010 0.0000 Sample 7 8 0.0073 0.0003 0.0007 Sample 4 8 0.0005 0.006 0.0001 Sample 8 7 0.236 0.0004 0.0023 Sample 10 7 0.0163 0.0009 0.0241 0.0013 0.0021 0.0006 Sample 9 7 0.0015 Sample 5 8 0.0006 0.0205 0.026 0.0003 0.0513 0.0007 0.0027 0.0003 0.0106 0.0002 Sample 3 8 0.0003 0.0044 0.0028 0.802 0.0008 -0.0013 0.0001 0.0135 -0.0004 0.0321 0.0295 0.003 0.0013 Sample 7 8 0.0146 0.0012 0.2366 0.0009 0.015 0.0062 -0.0032 0.0082 0.0460 0.0011 Sample 12 7 (0.0134 0.026 0.0037 0.0135 0.052 0.0040 0.0012 Vanadium Sample 1 7 O.0014 -0.0064 -0.0004 Sample 13 7 0.0013 0.0038 0.0003 0.0005 0.0009 0.0016 Sample 10 8 0.0008 0.0005 Sample 9 7 0.0006 Sample 5 7 (0.008 0.0008 Sample 11 7 0.004 0.0015 -0.0008 Sample 3 8 0.0017 0.0016 Tin Sample 1 7 0. Distributed under ASTM license by Beuth Verlag.0015 Sample 12 8 0.0094 0.0004 Sample 7 7 0.0007 Sample 8 5 0.0006 Sample 13 7 0.0002 0.0481 0.0009 -0.0012 0.0003 0.0011 0.0004 Sample 11 8 0.% Sample 12 8 0.0039 0.0015 0.008 0.0006 0.047 0.0298 0.0079 -0.0010 Sample 12 8 0.0020 -0.0049 0.0122 0.0002 0.01) 0.0028 0.0004 Sample 4 8 0.0005 0.0003 0.012 0.0061 -0.0047 0.0358 0.0006 Sample 9 7 0.0004 0.0004 Sample 3 8 0.0055 0.0003 0.0008 0.015 0.0022 Sample 2 7 0.0056 -0.0019 0.0029 0.0001 0.0052 Sample 13 7 0.0006 Sample 13 7 0.004 0.0003 Sample 7 8 0.001) 0.0006 Sample 2 7 0.034 0.0076 0.005 0.0135 0.0082 0.0007 0.0006 Sample 10 8 0.0006 Sample 12 8 0.0043 0.0144 0.0043 0.0024 0.012 0.8233 0.3044 0.002 0.0020 -0.0007 0.033 0.0001 0.0046 0.31 0.0076 0.0002 0.0403 0.0588 0.0001 0.015 0.0001 0.0007 Sample 12 8 (0.002) 0.0020 0. cO E415-15 TABLE2 Continued Number of Certified Material Xbar R Bias Laboratories Value.0016 0.0173 0.0003 0.0001 0.0007 0.0022 0.0019 Sample 9 7 0.0004 Sample 11 8 0.0022 0.0263 0.005 0.0003 Sample 7 8 0.0013 0.Q108 Sample 2 6 0.0096 O.0003 0.0046 0.002) 0.0019 Sample 4 7 0.0014 -0.0001 0.0004 Sample 5 7 (<0.0232 0.0047 Sample 3 7 0.0059 Titanium Sample 1 7 0.0213 Sample 8 7 0.0004 Sample 13 7 0.0017 Sample 10 8 0.0019 Sample 10 8 0.0028 0.0030 0.0018 Sample 6 8 0.0008 0.0002 0.0003 Sample 5 7 (0.0002 0.0007 0.005 0.0197 0.0024 0.0063 -0.0006 0.0031 -0.0156 0.0001 0.0221 0.0018 0.3322 0.0054 -0.001) 0.0008 0.0011 0.0004 Sample 11 8 0.0021 -0.0002 0.0006 10 Copyright ASTM International.0036 0.0018 Sample 8 7 (0.327 0.0006 Sample 5 7 0.061 0.008 0.0005 -0.0126 0.009 0.0020 0.0022 0.0410 Sample 2 7 0.0015 Sample 9 6 0.0064 0.0194 0.003 0.0004 Sample 2 7 0.0076 0.0010 0.0124 0.0010 0.0015 0.0009 0.003 0.0035 0.0005 0.0006) 0.0003 0.022 0.0034 Sample 4 8 0.0021 0.0012 -0.0006 Sample 6 8 0.025 0.0031 Zirconium Sample 1 6 (0.0034 Sample 13 6 0.0278 0.0010 0.0025 0.0112 -0.0023 -0.0001 0.054 0.016 0.0002 0.0046 0.Q1 0.0056 Sulfur Sample 1 7 0.0036 0.0127 0.Tel : +49 30 2601-2361 .01 0.0004 Sample 6 7 0.0001 0.0036 0.0010 Sample 11 8 0.0006 Sample 4 8 0.003 0.0234 0.0028 0. org).1 carbon steel. which you may attend. are entirely their own responsibility. or through the ASTM website (www.org (e-mail}.com/ 11 Copyright ASTM International. MA 01923. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised. at the address shown below. spark atomic emission.astm. Danvers. Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center. West Conshohocken. Distributed under ASTM license by Beuth Verlag.Tel : +49 30 2601-2361 . Your comments will receive careful consideration at a meeting of the responsible technical committee. http://www. 222 Rosewood Drive. low-alloy steel. If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards. PA 19428-2959. United States. 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